Spinning solutions for the manufacture of soft-luster rayon



g -1,987,095 SPINNING: SOLUTIONS FOR THE MANUFACam URE F 's FT L sTER RAYQN Iauao1ph;{s..'131 Elizabcthtongflfennf assignor L to'North' American Rayon..0orporation, New

" -York,: N;' Y., a corporationof Delaware I I '6 'Claims.i. (Cl. 10640) The present invention-relates to-a process-off:

preparing cellulosic spinning solutions from-which soft' luster filaments, yarns, ribbons, films,-' etc'.;

may be formed.

5" The primary objectofmy invention has to do with the incorporation of an organic titanium compound into cellulosic spinning solutions which, upon extrusion or molding, yieldsoft-luster cellulosic products. i r

Another object of my invention is theincorpora tion of an organic titaniumjcomp'ound 'composi-.

tion into viscose and cuprammonium spinning solutions, said composition consisting of (C2H5O) 2TiO.PH304 dissolved and/or dispersed in an organic liquid inert to said spinning solution.

Other objects of my invention will become apparent to those skilled in the art after a study of the following specification.

In the early days of rayon manufacture, the demand was entirely for yarns having the highest possible degree of luster. Later, when it was found that highly lustrous rayon too clearly indicated its origin-an artificial fibera demand arose for artificial silk which more closely approximated to natural silk. The earliest attempt to meet the demand of dull-luster viscose yarn, for example,

was a method of retaining sulphur particles inthe fibers by discontinuing the normal desulphurizing step during its manufacture. Although this yarn showed decreased luster, due to scattering of light by the sulphur particles, it was impermanent and exhibited an unattractive bloom. This method has been improved by dispersing, instead of sulphur, fine inorganic or organic particles in cellulosic spinning solutions, such as pigments, hydrocarbons and the like.

I am well aware that it has, heretofore, been proposed to incorporate inorganic and organic titanium compounds into cellulosic spinning solutions to produce soft-luster yarns (vide U. S. Patents 1,692,372 and 1,791,199 to Gardner, U. S. Patent 1,875,894 to Singmaster, U. S. Patent 1,969,689 to Byron, British Patent 343,949 to Dreyfus, etc.)

With exception of a special titanium oxalate, disclosed in the aforementioned U. S. Patent 1,969,689, to Thomas H. Byron of August 7, 1934, all of the titanium compounds, heretofore used in the art, are somewhat alkaliand acid-soluble. For this reason considerable amounts of these titanium compounds are wasted during the manufacture of soft-luster rayon.

In accordance with my present invention, not a titanium oxalate but a titanium compound having the rdrmma}(cznsoirrio-rii is"used combination with viscose'. 'and cuprammonium f This titanium "compound may be by,

reacting TiPCls or TiRClvO uponaliphagtic alcohols' toform intermediate compounds havingjthe'struc- (GHO) aTiClLPHz'OIan'd Cz I-lj50). z'I iC 1.PHzOi, respectively. After hydrolyain'g" thesegum-like intermediates, an organictitaniumcompound is obtainedfhaving'the formula:

(cz'nsoimornsoi,

which is soluble in alcohol, insoluble in water and ether, insoluble in viscose and cuprammonium cellulose solutions as well as in the acid setting baths used in connection with such spinning solutions.

The compound, before being dispersed in the cellulosic solutions, is finely ground in pebble or colloid mills. Instead of dispersing the titanium compound per se in the spinning solutions, it may first b'edissolved or dispersed in an inert, organic liquid to accelerate its uniform distribution there.- in. Thus, the titanium compoundmay be dissolved in alcohols and, subsequently, the alcoholic cellulose solutions to forni after extrusion; soft? 'lust'er,-cellulosic products.

solution added to the spinning solution. Due to.

' agents per se. It is to be noted,- however, that only such organic liquids are suitable which are inert with respect to the spinning solutions and which do not deleteriously affect the final products.

' The amounts of titanium compound added toa spinning solution may be varied practically at will, although I have found that additions of about 1 to 12% of (C2H5O) 2TiO.PI-I3O4 are surficient to produce soft-luster products. 7

Example 1 From 1 to 12% of (CzHsO) 2TiO.PH304, calcu, lated on the cellulose content, are added to a conventional viscose spinning solution in the form of a fine dispersion. The titanium compound may be I persedin the viscose solution, or it may be dissolved in an organic solvent prior to incorporation into said solution. Instead of dissolving thetitan ium compound, it may be ground and dispersed in f an inert, organic liquid'to form an organosol.

Thisorganosol is then emulsified with the viscose solution under continuous stirring; 'Iheloaded spinning solution is subsequently extruded into conventional spinning baths. c 1

Example 2 added to a conventional cuprammonium cellulose solution, the percentages of titanium compound being based upon its cellulose content." The V said percentages of titanium compound being I titanium compound is incorporated -tinto gthe cuprammonium cellulose solution in accordance with the methods set forth in Example 1.

It is to be emphasized that the amountsof titanium compound, set forth above, maybe decreased or increased. to vary', the luster of the finished, vcellulosic products, although excessive additions tend to weaken the tensile strength of the rayon and to clogthefine holes of the spin- -ning nozzles- Modifications may be made in details of the method and the product without departing from the spirit and scope of my invention as defined by the appended claims.

1'. A spinning solution for the manufacture of soft-luster products comprising a solution of the group consisting of viscose and cuprammonium cellulose, an organic liquid inert to said solution,

and an organic titanium compound having the 35A spinning solution for the manufacture of soft-lusterproductscomprising a solution of the I I r r grfoup" consisting tof viscose and cuprammonium- From 1 to 12% 0f (CzHsO) 2TiO.PI-I3O4 are cellulose and from 1 to 12 per cent of an organic titanium compound having the formula (c nsoig'riormol,

vcalculated on the cellulose content of the solution. i 4. A spinning solution for the manufacture of soft-luster products comprising a solution of the i group-consisting of viscose and cuprammonium cellulose an organic liquid inert to'said solution compound having the formula (c2350) z'riormoy v and from 1 to-t12 per cent of an" organic titanium.

jsa idi'jpercentages of titanium I compound being calculated onthe cellulose content of the solution.

5. A viscose filament containing finelydivided (C2H5 O) 2TiO.PH304. V 1

R DOLPH s. BLEY. I

. t a 30 1- 6. Acuprammonium filament containingfinely divided (CzHsO) 2TiO.PH304. 

